Hexaamminechromium(III) di­aqua­tetra­chloro­sodium(I)

Alig, E.; Fink, L.; Bolte, M.

doi:10.1107/S160053680302378X

Hexaamminechromium(III) diaquatetrachlorosodium(I)

The title compound, hexaamminechromium(III) diaquatetrachlorosodium(I), [Cr(NH₃)₆][NaCl₄(H₂O)₂], is composed of discrete [Cr(NH₃)₆]³⁺ cations and [NaCl₄(H₂O)₂]^3- anions. The Cr and Na ions are octahedrally coordinated. The crystal packing is characterized by an alternating arrangement of anions and cations and is stabilized by numerous hydrogen bonds.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680302378X/lh6127sup1.cif Contains datablocks I, global
	Structure factor file (CIF format) https://doi.org/10.1107/S160053680302378X/lh6127Isup2.hkl Contains datablock I

checkCIF report

Key indicators

Single-crystal X-ray study
T = 173 K
Mean (Cr-N) = 0.004 Å
R factor = 0.037
wR factor = 0.073
Data-to-parameter ratio = 15.2

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low .......       0.93

Alert level B
CHEMS01_ALERT_1_B  The sum formula contains elements in the wrong order.
            H  precedes Cl
            Sequence must be C, H, then alphabetical.

Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT420_ALERT_2_C D-H Without Acceptor       N6     -   H6C    ...          ?
PLAT731_ALERT_1_C Bond    Calc     0.88(3), Rep   0.881(10) ......       3.00 su-Rat
              N1   -H1A     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.88(4), Rep   0.873(10) ......       4.00 su-Rat
              N2   -H2B     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.88(3), Rep   0.875(10) ......       3.00 su-Rat
              N2   -H2C     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.88(3), Rep   0.877(10) ......       3.00 su-Rat
              N3   -H3A     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.88(3), Rep   0.875(10) ......       3.00 su-Rat
              N4   -H4A     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.87(3), Rep   0.877(10) ......       3.00 su-Rat
              N5   -H5C     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.87(3), Rep   0.874(10) ......       3.00 su-Rat
              N6   -H6C     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.84(3), Rep   0.837(10) ......       3.00 su-Rat
              O1   -H1E     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.84(3), Rep   0.836(10) ......       3.00 su-Rat
              O2   -H2E     1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.88(3), Rep   0.881(10) ......       3.00 su-Rat
              N1   -H1A     1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.88(4), Rep   0.873(10) ......       4.00 su-Rat
              N2   -H2B     1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.88(3), Rep   0.875(10) ......       3.00 su-Rat
              N2   -H2C     1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.88(3), Rep   0.875(10) ......       3.00 su-Rat
              N2   -H2C     1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.88(3), Rep   0.877(10) ......       3.00 su-Rat
              N3   -H3A     1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.88(3), Rep   0.875(10) ......       3.00 su-Rat
              N4   -H4A     1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.87(3), Rep   0.877(10) ......       3.00 su-Rat
              N5   -H5C     1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.87(3), Rep   0.874(10) ......       3.00 su-Rat
              N6   -H6C     1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.84(3), Rep   0.837(10) ......       3.00 su-Rat
              O1   -H1E     1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.84(3), Rep   0.836(10) ......       3.00 su-Rat
              O2   -H2E     1.555   1.555
PLAT736_ALERT_1_C H...A   Calc     2.43(4), Rep   2.426(14) ......       2.86 su-Rat
              H2B  -CL1     1.555   4.466
PLAT736_ALERT_1_C H...A   Calc     2.49(3), Rep   2.487(14) ......       2.14 su-Rat
              H3B  -CL2     1.555   2.665

Alert level G
REFLT03_ALERT_1_G ALERT: Expected hkl max differ from CIF values
           From the CIF: _diffrn_reflns_theta_max           27.12
           From the CIF: _reflns_number_total               2941
           From the CIF: _diffrn_reflns_limit_ max hkl    8.   10.   27.
           From the CIF: _diffrn_reflns_limit_ min hkl   -9.  -10.  -27.
           TEST1: Expected hkl limits for theta max
           Calculated maximum hkl    9.   11.   29.
           Calculated minimum hkl   -9.  -11.  -29.
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
            correct. If it is not, please give the correct count in the
            _publ_section_exptl_refinement section of the submitted CIF.
           From the CIF: _diffrn_reflns_theta_max           27.12
           From the CIF: _reflns_number_total               2941
           Count of symmetry unique reflns         1880
           Completeness (_total/calc)            156.44%
           TEST3: Check Friedels for noncentro structure
           Estimate of Friedel pairs measured      1061
           Fraction of Friedel pairs measured     0.564
           Are heavy atom types Z>Si present          yes

   1 ALERT level A = In general: serious problem
   1 ALERT level B = Potentially serious problem
  24 ALERT level C = Check and explain
   2 ALERT level G = General alerts; check

  25 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   1 ALERT type 2 Indicator that the structure model may be wrong or deficient
   1 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Siemens, 1995); cell refinement: SMART; data reduction: SAINT (Siemens, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 1991); software used to prepare material for publication: SHELXL97.

Hexaamminechromium(III) diaquatetrachlorosodium(I) top

Crystal data top

H₁₈CrN₆³⁺·H₄Cl₄NaO₂³⁻	F(000) = 732
M_r = 355.03	D_x = 1.612 Mg m⁻³
Orthorhombic, P2₁2₁2₁	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ac 2ab	Cell parameters from 5893 reflections
a = 7.0596 (3) Å	θ = 1–25°
b = 9.1575 (4) Å	µ = 1.53 mm⁻¹
c = 22.631 (1) Å	T = 173 K
V = 1463.06 (11) Å³	Plate, orange
Z = 4	0.34 × 0.12 × 0.06 mm

Data collection top

Siemens CCD three-circle diffractometer	2941 independent reflections
Radiation source: fine-focus sealed tube	2340 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.062
ω scans	θ_max = 27.1°, θ_min = 1.8°
Absorption correction: empirical (SADABS; Sheldrick, 1996)	h = −9→8
T_min = 0.624, T_max = 0.914	k = −10→10
14937 measured reflections	l = −27→27

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.037	Only H-atom coordinates refined
wR(F²) = 0.073	w = 1/[σ²(F_o²) + (0.0304P)² + 0.4093P] where P = (F_o² + 2F_c²)/3
S = 1.06	(Δ/σ)_max = 0.001
2941 reflections	Δρ_max = 0.41 e Å⁻³
194 parameters	Δρ_min = −0.43 e Å⁻³
22 restraints	Absolute structure: Flack (1983), 0000 Friedel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.18 (3)

Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Cr1	0.59753 (10)	0.59589 (6)	0.87758 (2)	0.01310 (14)
N1	0.8049 (5)	0.5294 (4)	0.93629 (16)	0.0201 (8)
H1A	0.894 (4)	0.595 (3)	0.9420 (18)	0.030*
H1B	0.859 (5)	0.445 (2)	0.9312 (17)	0.030*
H1C	0.775 (7)	0.526 (4)	0.9739 (7)	0.030*
N2	0.3845 (6)	0.5288 (4)	0.93486 (16)	0.0203 (7)
H2A	0.420 (6)	0.511 (4)	0.9714 (8)	0.030*
H2B	0.298 (5)	0.596 (4)	0.9401 (18)	0.030*
H2C	0.329 (5)	0.451 (3)	0.9204 (17)	0.030*
N3	0.3916 (6)	0.6643 (4)	0.81852 (14)	0.0186 (7)
H3A	0.286 (3)	0.616 (4)	0.8247 (17)	0.028*
H3B	0.427 (6)	0.636 (4)	0.7833 (8)	0.028*
H3C	0.371 (6)	0.7582 (14)	0.8190 (17)	0.028*
N4	0.8059 (5)	0.6616 (4)	0.81882 (16)	0.0193 (8)
H4A	0.902 (4)	0.601 (4)	0.8191 (17)	0.029*
H4B	0.778 (6)	0.670 (5)	0.7812 (7)	0.029*
H4C	0.847 (6)	0.749 (2)	0.8273 (17)	0.029*
N5	0.5928 (6)	0.3919 (3)	0.83651 (14)	0.0187 (7)
H5A	0.624 (6)	0.412 (4)	0.8000 (7)	0.028*
H5B	0.475 (2)	0.361 (4)	0.8379 (17)	0.028*
H5C	0.666 (4)	0.328 (3)	0.8539 (15)	0.028*
N6	0.5999 (6)	0.7992 (3)	0.91872 (14)	0.0206 (7)
H6A	0.595 (7)	0.792 (4)	0.9576 (5)	0.031*
H6B	0.717 (2)	0.830 (4)	0.9181 (18)	0.031*
H6C	0.512 (4)	0.860 (4)	0.9072 (17)	0.031*
Na1	0.6003 (3)	0.40765 (16)	0.12594 (6)	0.0228 (3)
Cl1	0.60018 (16)	0.68763 (10)	0.06311 (4)	0.0213 (2)
Cl3	0.59675 (17)	0.11893 (10)	0.17514 (4)	0.0234 (2)
Cl2	0.91942 (16)	0.47705 (10)	0.19570 (4)	0.0205 (2)
Cl4	0.27215 (15)	0.34262 (11)	0.06183 (4)	0.0228 (2)
O1	0.8203 (4)	0.3253 (5)	0.05777 (16)	0.0373 (9)
H1D	0.9384 (16)	0.332 (6)	0.058 (2)	0.056*
H1E	0.787 (7)	0.282 (5)	0.0269 (13)	0.056*
O2	0.3804 (5)	0.5098 (3)	0.19172 (13)	0.0292 (7)
H2D	0.397 (7)	0.526 (5)	0.2279 (7)	0.044*
H2E	0.273 (3)	0.477 (5)	0.183 (2)	0.044*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cr1	0.0146 (3)	0.0105 (3)	0.0141 (3)	−0.0003 (3)	−0.0001 (3)	−0.0002 (2)
N1	0.026 (2)	0.0143 (18)	0.0202 (18)	0.0029 (15)	−0.0074 (18)	−0.0029 (18)
N2	0.022 (2)	0.0172 (18)	0.0216 (17)	0.0005 (17)	0.000 (2)	0.0016 (16)
N3	0.0194 (19)	0.0155 (17)	0.0210 (17)	0.003 (2)	−0.0016 (19)	0.0025 (15)
N4	0.022 (2)	0.0156 (18)	0.0200 (18)	0.0014 (17)	0.0021 (17)	0.0002 (17)
N5	0.0223 (19)	0.0146 (17)	0.0192 (16)	0.0001 (19)	−0.0047 (18)	0.0003 (14)
N6	0.024 (2)	0.0160 (17)	0.0218 (17)	0.0028 (19)	−0.0067 (19)	−0.0034 (14)
Na1	0.0227 (7)	0.0218 (7)	0.0240 (7)	0.0010 (8)	0.0005 (8)	−0.0012 (6)
Cl1	0.0213 (5)	0.0190 (5)	0.0235 (5)	−0.0009 (5)	−0.0010 (5)	0.0023 (4)
Cl3	0.0217 (5)	0.0199 (5)	0.0285 (5)	0.0005 (5)	−0.0004 (5)	0.0051 (4)
Cl2	0.0236 (6)	0.0196 (5)	0.0183 (5)	−0.0027 (5)	−0.0011 (5)	0.0012 (4)
Cl4	0.0269 (6)	0.0193 (5)	0.0221 (5)	−0.0023 (5)	−0.0008 (5)	0.0005 (4)
O1	0.0286 (18)	0.050 (2)	0.0329 (19)	−0.0022 (18)	0.0029 (18)	−0.0169 (17)
O2	0.0263 (18)	0.0393 (18)	0.0222 (16)	0.0022 (17)	−0.0041 (16)	−0.0038 (14)

Geometric parameters (Å, º) top

Cr1—N1	2.069 (4)	N4—H4C	0.876 (10)
Cr1—N3	2.072 (4)	N5—H5A	0.875 (10)
Cr1—N4	2.072 (4)	N5—H5B	0.880 (10)
Cr1—N2	2.079 (4)	N5—H5C	0.877 (10)
Cr1—N6	2.082 (3)	N6—H6A	0.883 (10)
Cr1—N5	2.087 (3)	N6—H6B	0.876 (10)
N1—H1A	0.881 (10)	N6—H6C	0.874 (10)
N1—H1B	0.874 (10)	Na1—O1	2.316 (4)
N1—H1C	0.878 (10)	Na1—O2	2.345 (4)
N2—H2A	0.878 (10)	Na1—Cl4	2.797 (2)
N2—H2B	0.873 (10)	Na1—Cl2	2.824 (2)
N2—H2C	0.875 (10)	Na1—Cl3	2.8690 (17)
N3—H3A	0.877 (10)	Na1—Cl1	2.9318 (17)
N3—H3B	0.873 (10)	O1—H1D	0.836 (10)
N3—H3C	0.872 (10)	O1—H1E	0.837 (10)
N4—H4A	0.875 (10)	O2—H2D	0.840 (10)
N4—H4B	0.877 (10)	O2—H2E	0.836 (10)

N1—Cr1—N3	179.40 (17)	Cr1—N4—H4C	111 (3)
N1—Cr1—N4	89.72 (16)	H4A—N4—H4C	109 (4)
N3—Cr1—N4	89.79 (13)	H4B—N4—H4C	102 (4)
N1—Cr1—N2	91.41 (13)	Cr1—N5—H5A	103 (3)
N3—Cr1—N2	89.08 (16)	Cr1—N5—H5B	107 (3)
N4—Cr1—N2	178.66 (16)	H5A—N5—H5B	110 (4)
N1—Cr1—N6	88.30 (14)	Cr1—N5—H5C	113 (3)
N3—Cr1—N6	91.37 (14)	H5A—N5—H5C	114 (4)
N4—Cr1—N6	91.25 (15)	H5B—N5—H5C	109 (4)
N2—Cr1—N6	89.49 (15)	Cr1—N6—H6A	112 (3)
N1—Cr1—N5	91.94 (14)	Cr1—N6—H6B	107 (3)
N3—Cr1—N5	88.39 (14)	H6A—N6—H6B	95 (4)
N4—Cr1—N5	89.16 (14)	Cr1—N6—H6C	116 (3)
N2—Cr1—N5	90.09 (14)	H6A—N6—H6C	108 (4)
N6—Cr1—N5	179.52 (19)	H6B—N6—H6C	118 (4)
Cr1—N1—H1A	114 (3)	O1—Na1—O2	175.42 (15)
Cr1—N1—H1B	119 (3)	O1—Na1—Cl4	98.07 (10)
H1A—N1—H1B	108 (4)	O2—Na1—Cl4	82.30 (10)
Cr1—N1—H1C	118 (3)	O1—Na1—Cl2	84.88 (10)
H1A—N1—H1C	93 (4)	O2—Na1—Cl2	94.79 (9)
H1B—N1—H1C	102 (4)	Cl4—Na1—Cl2	177.03 (7)
Cr1—N2—H2A	116 (3)	O1—Na1—Cl3	87.94 (12)
Cr1—N2—H2B	112 (3)	O2—Na1—Cl3	96.63 (9)
H2A—N2—H2B	102 (4)	Cl4—Na1—Cl3	89.88 (5)
Cr1—N2—H2C	109 (3)	Cl2—Na1—Cl3	89.85 (5)
H2A—N2—H2C	109 (4)	O1—Na1—Cl1	87.82 (12)
H2B—N2—H2C	108 (4)	O2—Na1—Cl1	87.65 (9)
Cr1—N3—H3A	110 (3)	Cl4—Na1—Cl1	86.24 (5)
Cr1—N3—H3B	107 (3)	Cl2—Na1—Cl1	94.28 (5)
H3A—N3—H3B	104 (4)	Cl3—Na1—Cl1	173.80 (6)
Cr1—N3—H3C	114 (3)	Na1—O1—H1D	130 (4)
H3A—N3—H3C	111 (4)	Na1—O1—H1E	122 (4)
H3B—N3—H3C	110 (4)	H1D—O1—H1E	108 (5)
Cr1—N4—H4A	111 (3)	Na1—O2—H2D	127 (4)
Cr1—N4—H4B	119 (3)	Na1—O2—H2E	108 (3)
H4A—N4—H4B	103 (4)	H2D—O2—H2E	114 (5)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···Cl1ⁱ	0.88 (1)	2.47 (2)	3.325 (4)	165 (4)
N1—H1B···Cl4ⁱⁱ	0.87 (1)	2.71 (3)	3.415 (4)	139 (3)
N1—H1C···O1ⁱⁱⁱ	0.88 (1)	2.66 (3)	3.326 (6)	133 (3)
N1—H1C···Cl1ⁱⁱⁱ	0.88 (1)	2.79 (3)	3.525 (4)	142 (3)
N2—H2A···Cl1ⁱⁱⁱ	0.88 (1)	2.92 (3)	3.586 (4)	134 (3)
N2—H2A···Cl4ⁱⁱⁱ	0.88 (1)	2.77 (3)	3.434 (4)	134 (4)
N2—H2B···Cl1^iv	0.87 (1)	2.43 (1)	3.282 (4)	167 (4)
N2—H2C···Cl3^v	0.88 (1)	2.79 (3)	3.486 (4)	138 (3)
N2—H2C···O1^v	0.88 (1)	2.58 (3)	3.278 (5)	137 (3)
N3—H3A···Cl3^v	0.88 (1)	2.53 (2)	3.329 (4)	151 (4)
N3—H3B···Cl2^vi	0.87 (1)	2.49 (1)	3.344 (4)	167 (4)
N3—H3C···Cl2^iv	0.87 (1)	2.47 (2)	3.306 (3)	161 (4)
N4—H4A···Cl3ⁱⁱ	0.88 (1)	2.44 (2)	3.291 (4)	164 (4)
N4—H4B···Cl2^vi	0.88 (1)	2.74 (3)	3.450 (4)	139 (4)
N4—H4C···O2ⁱ	0.88 (1)	2.26 (2)	3.064 (5)	153 (4)
N5—H5B···Cl3^v	0.88 (1)	2.69 (2)	3.513 (4)	156 (4)
N5—H5A···Cl2^vi	0.88 (1)	2.59 (2)	3.406 (3)	156 (4)
N5—H5C···Cl4ⁱⁱ	0.88 (1)	2.58 (2)	3.392 (3)	156 (3)
N6—H6A···Cl1ⁱⁱⁱ	0.88 (1)	2.57 (2)	3.424 (3)	162 (3)
N6—H6B···Cl1ⁱ	0.88 (1)	2.74 (2)	3.558 (4)	156 (4)
N6—H6C···Cl2^iv	0.87 (1)	2.84 (3)	3.539 (3)	138 (3)
O1—H1D···Cl4^vii	0.84 (1)	2.36 (1)	3.195 (3)	177 (6)
O1—H1E···Cl4^viii	0.84 (1)	2.31 (2)	3.131 (4)	167 (5)
O2—H2D···Cl3^ix	0.84 (1)	2.35 (2)	3.179 (3)	167 (4)
O2—H2E···Cl2^x	0.84 (1)	2.51 (3)	3.269 (4)	151 (4)

Symmetry codes: (i) x+1/2, −y+3/2, −z+1; (ii) x+1/2, −y+1/2, −z+1; (iii) x, y, z+1; (iv) x−1/2, −y+3/2, −z+1; (v) x−1/2, −y+1/2, −z+1; (vi) −x+3/2, −y+1, z+1/2; (vii) x+1, y, z; (viii) x+1/2, −y+1/2, −z; (ix) −x+1, y+1/2, −z+1/2; (x) x−1, y, z.

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Hexaamminechromium(III) di­aqua­tetra­chloro­sodium(I)

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Hexaamminechromium(III) diaquatetrachlorosodium(I)